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用于评估活性药物成分造假的同位素13C核磁共振光谱法:阿司匹林和对乙酰氨基酚的特定位置13C含量

Isotopic 13C NMR spectrometry to assess counterfeiting of active pharmaceutical ingredients: site-specific 13C content of aspirin and paracetamol.

作者信息

Silvestre Virginie, Mboula Vanessa Maroga, Jouitteau Catherine, Akoka Serge, Robins Richard J, Remaud Gérald S

机构信息

University of Nantes-CNRS, Chemistry and Interdisciplinarity: Synthesis, Analysis and Modeling, UMR6230, 2 rue de la Houssinière, BP 92208, F-44322 Nantes cedex 3, France.

出版信息

J Pharm Biomed Anal. 2009 Oct 15;50(3):336-41. doi: 10.1016/j.jpba.2009.04.030. Epub 2009 May 7.

Abstract

Isotope profiling is a well-established technique to obtain information about the chemical history of a given compound. However, the current methodology using IRMS can only determine the global (13)C content, leading to the loss of much valuable data. The development of quantitative isotopic (13)C NMR spectrometry at natural abundance enables the measurement of the (13)C content of each carbon within a molecule, thus giving simultaneous access to a number of isotopic parameters. When it is applied to active pharmaceutical ingredients, each manufactured batch can be characterized better than by IRMS. Here, quantitative isotopic (13)C NMR is shown to be a very promising and effective tool for assessing the counterfeiting of medicines, as exemplified by an analysis of aspirin (acetylsalicylic acid) and paracetamol (acetaminophen) samples collected from pharmacies in different countries. It is proposed as an essential complement to (2)H NMR and IRMS.

摘要

同位素剖析是一种成熟的技术,用于获取有关给定化合物化学历史的信息。然而,当前使用同位素比质谱仪(IRMS)的方法只能确定整体的¹³C含量,导致许多有价值的数据丢失。天然丰度下定量同位素¹³C核磁共振光谱法的发展使得能够测量分子内每个碳原子的¹³C含量,从而可同时获取多个同位素参数。当将其应用于活性药物成分时,每个生产批次都能比使用IRMS得到更好的表征。在此,定量同位素¹³C核磁共振被证明是评估药品假冒的一种非常有前景且有效的工具,从对从不同国家药店收集的阿司匹林(乙酰水杨酸)和对乙酰氨基酚(扑热息痛)样品的分析中可见一斑。它被提议作为²H核磁共振和IRMS的重要补充。

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